EXPERIMENT 5: GAS CHROMATOGRAPHY (GC)

OBJECTIVES:

1. To discover the retention times tR for n-butanol and methanol.

2. To determine the components in a standard mixture based on the tR.

INTRODUCTION

Gas chromatography (GC) is a type of chromatography that can be vaporized without

decomposition in analytical chemistry for the separation and analysis of compounds. GC is
usually used to test the purity of a specific substance or separating the various components of
a mixture. GC is also used to identify a compound.

The mobile phase of GC is usually inert gas such as helium or unreactive gas such as
nitrogen. Helium remains the most widely used carrier gas in approximately 90 percent of the
instruments, although hydrogen is preferred for improved separations. The stationary phase is
a microscopic layer of liquid or polymer on an inert solid support, inside a piece of glass or
metal tubing called a column.

A sample port is required to insert the sample in the top of the column. Modern injection
technology often uses heated sample ports to inject and vaporize the sample in an almost
simultaneous manner. A calibrated microsyringe is used to deliver the sample volume to the
vaporization chamber in the range of a few microliters via a rubber septum.

A detector is a device at the end of the column that measures the components of the mixture
quantitatively when they elude in combination with carrier gas. Every detector has two main
parts that serve as transducers for converting the detected property changes to an electrical
signal recorded as a chromatogram when used together. An ideal GC detector is characterized
by a number of features which includes universal response, high sensitivity, reproducible
results, large linear dynamic range, fast response time and non-destructive.

There are many types of detector for GC. For example Mass Spectrometer (MS), Flame
Ionization (FID), Thermal Conductivity (TCD), Electron-Capture (ECD), Atomic Emission
(AED), Chemiluminescence (CS) and Photoionization (PID). The usage of detector depends
on the sample for example FID are used to detect organic compounds while ECD are used to
detect halogenated hydrocarbons.

APPARATUS

1. Syringe
2. Beaker
3. Dropper

CHEMICALS

1. Methanol
2. n-butanol
3. Standard mixture of methanol and n-butanol and methanol (1:1 ratio)
4. Unknown sample.
RESULTS:
a) Data:
Table 5.1: Retention Time and Peak Area of Sample
Samples Temperature ( 0C) Retention Time, tR Peak Area (%)
(min)
Methanol 70 1.931 99.88
n-butanol 70 2.917 99.88
Standard mixture:
Compound 1 70 2.841 75.17
Compound 2 70 1.924 24.80
Unknown sample 70 1.929 96.95
DISCUSSIONS:
Based on the experiment, Gas Chromatography (GC) was examined which includes the
concepts of retention time, the components of GC and the concept of resolution by using
methanol, n-butanol, standard mixture of methanol with n-butanol, and an unknown sample.

The brand of the Gas chromatograph used in this experiment was Agilent7820A with an
autosampler. Agilent7820A is high-quality GC with a wide range of inlet and detector
options, including mass spectrometer.

Retention time (tR) is a measure of the time taken for solute to pass through a
chromatography column. It is calculated as the time from injection to detection. The
separation of sample components from a GC column depends on how long each individual
component moves and elutes from the column. The retention time detected in this experiment
for methanol, n-butanol, Standard mixture compound 1, Standard mixture compound 2, and
unknown sample are 1.931, 2.917, 2.841, 1.924, and 1.929 with a peak area of 99.88%,
99.88%, 75.17%, 24.80% and 96.95% respectively. In this experiment, methanol and
standard mixture compound 2 have the fastest retention time meaning both of the compounds
eluted first.

Using GC, a compound can be identified from a mixture of compounds by its retention
time. The retention time for unknown sample and methanol is almost the same meaning that
the unknown sample is methanol. This also applies to the standard mixture which have the
retention time of 1.924 and 2.841 which is similar to methanol and n-butanol which were
1.931 and 2.917 respectively thus the standard mixture is a mixture of methanol and n-
butanol.

In this experiment, the detector used in the GC was Flame Ionization Detector (FID)
because the compounds used in this experiments were organic hydrocarbons. FID are used in
this experiment because it’s a good general detector for organic compounds and is able to
detect at the nanogram level.
QUESTIONS

1. State the types of compounds which are suitable for analysis using GC.

2. Why is FID a suitable detector for this analysis?

FID stands for Flame-ionization detector (FID) which are used to detect organic compounds
which are used in this experiment.

3. List two factors which can increase the efficiency of a GC column.

 Column pressure
 Column diameter.
METHODOLOGY